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Preparation method of griseofulvin

A technology of griseofulvin and acetone, which is applied in the field of griseofulvin preparation, can solve the problems of power, energy waste, increased production cost, and large loss of solvent, so as to save energy, reduce the number of crystallization times, and reduce production costs Effect

Active Publication Date: 2014-09-03
内蒙古格林特制药有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are two crystallization processes in the process steps of this method, which leads to a lot of yield loss in the double crystallization process, low yield of finished product, large loss of solvent, waste of power and energy, and increase of production cost.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Example 1 A preparation method of griseofulvin, comprising the following steps:

[0014] A. Heating the griseofulvin fermentation broth to 80°C, adding calcium oxide to adjust the pH to 5.5, separating the solid and liquid from the plate and frame, adding calcium oxide to the filter cake to granulate, and extracting with acetone to obtain the griseofulvin acetone extract;

[0015] B. Griseofulvin acetone extract is decolorized by activated carbon column to obtain griseofulvin acetone decolorization solution, and the decolorization solution enters the concentration tank, and decompresses by circulating steam in the jacket and vacuumizing the tank to reduce the boiling point of acetone Concentration, the concentration temperature is controlled at 27 oC , the vacuum degree is controlled at -0.09MPa. After concentration, the acetone evaporates rapidly, is cooled and recovered, and recycled, and the crystals are naturally precipitated. Under vacuum conditions, filter the ...

Embodiment 2

[0018] Example 2 A preparation method of griseofulvin, comprising the following steps:

[0019] A. Heating the griseofulvin fermentation broth to 100°C, adding calcium oxide to adjust the pH to 6, separating the solid and liquid from the plate and frame, adding calcium oxide to the filter cake to granulate, and extracting with acetone to obtain the griseofulvin acetone extract;

[0020] B. Griseofulvin acetone extract is decolorized by activated carbon column to obtain griseofulvin acetone decolorization solution, and the decolorization solution enters the concentration tank, and decompresses by circulating steam in the jacket and vacuumizing the tank to reduce the boiling point of acetone Concentration, the concentration temperature is controlled at 24 o C. The vacuum degree is controlled at -0.07MPa. After concentration, the acetone evaporates rapidly, is cooled and recovered, and recycled, and the crystals are naturally precipitated. When the acetone is not completely eva...

Embodiment 3

[0023] Example 3 A preparation method of griseofulvin, comprising the following steps:

[0024] A. Heat the griseofulvin fermentation broth to 90°C, add calcium oxide to adjust the pH to 6.5, separate the plate and frame from solid and liquid, add calcium oxide to the filter cake to granulate, and extract with acetone to obtain the griseofulvin acetone extract;

[0025] B. Griseofulvin acetone extract is decolorized by activated carbon column to obtain griseofulvin acetone decolorization solution, and the decolorization solution enters the concentration tank, and decompresses by circulating steam in the jacket and vacuumizing the tank to reduce the boiling point of acetone Concentration, the concentration temperature is controlled at 30 oC , the vacuum degree is controlled at -0.08MPa. After concentration, the acetone evaporates rapidly, is cooled and recovered, and recycled, and the crystals are naturally precipitated. Under vacuum conditions, filter the concentrated ...

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PUM

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Abstract

The invention discloses a preparation method of griseofulvin, which is composed of the following steps: A, heating the griseofulvin fermented liquid, adding calcium oxide to adjust the pH, separating the solid and liquid from the plate and frame, adding calcium oxide to the filter cake to granulate, Extract with acetone to obtain griseofulvin acetone extract; B. Griseofulvin acetone extract is decolorized by activated carbon column to obtain griseofulvin acetone decolorization liquid, and the decolorization liquid enters the concentration tank, concentrates and crystallizes to obtain griseofulvin wet crystals C, griseofulvin wet crystals are washed once with dichloromethane and ethanol mixed solution under stirring, and then washed once with the medicinal ethanol of 95% with concentration under stirring, dried in a vacuum drier, ultrafinely pulverized, Get griseofulvin products. Compared with the traditional preparation method, the present invention reduces the number of crystallization times in the process of preparing griseofulvin in the prior art, effectively avoids the yield loss caused by the recrystallization of griseofulvin, and can increase the total yield of griseofulvin Increased by 7 to 10%, greatly reducing production costs.

Description

technical field [0001] The invention relates to a preparation method of a raw material drug, in particular to a preparation method of griseofulvin. Background technique [0002] Griseofulvin is an antibiotic raw material drug. Its English name is Griseofulvin. Its Chinese aliases are griseofulvin and microcrystalline griseofulvin. 07-8, this product is white or off-white fine powder; this product mainly has good antibacterial effect on superficial fungi such as Trichophyton, Microsporum, and Epidermophyton. [0003] Griseofulvin is indicated for the treatment of various tinea conditions, including tinea capitis, tinea barbae, tinea corporis, jock itch, tinea pedis and onychomycosis. [0004] At present, the method for preparing griseofulvin generally comprises the following steps: a: heating with griseofulvin fermented liquid, solid-liquid separation in plates and frames, filter cake granulation, acetone extraction to obtain griseofulvin acetone extract; b, The griseofulvi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/94
Inventor 胡志远赵一楠涂顺根胡佳悦涂书宋淼徐思张士军李国平
Owner 内蒙古格林特制药有限责任公司
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